# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_403_autored
_database_code_depnum_ccdc_archive 'CCDC 2237885'
loop_
_audit_author_name
_audit_author_address
'Juntaro Nogami'
;Tokyo Institute of Technology
Japan
;
_audit_update_record             
;
2023-01-25 deposited with the CCDC.	2023-03-10 downloaded from the CCDC.
;
_audit_creation_date             2023-01-17
_audit_creation_method           
;
Olex2 1.5-ac5-023
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            (+-)-3a
_chemical_name_systematic        '[2.2]Triphenylenophane'
_chemical_formula_moiety         'C58 H46 N2 O6 S2'
_chemical_formula_sum            'C58 H46 N2 O6 S2'
_chemical_formula_weight         931.09
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C232 H184 N8 O24 S8 '
_chemical_oxdiff_usercomment     200K
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.3238(6)
_cell_length_b                   20.1104(7)
_cell_length_c                   16.9292(7)
_cell_angle_alpha                90
_cell_angle_beta                 96.463(4)
_cell_angle_gamma                90
_cell_volume                     4507.3(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9694
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      29.4010
_cell_measurement_theta_min      1.8740
_shelx_estimated_absorpt_T_max   0.984
_shelx_estimated_absorpt_T_min   0.929
_exptl_absorpt_coefficient_mu    0.177
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.955
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.61a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1952
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-19 0 -1 0.0360
18 0 2 0.0601
-1 -28 3 0.0904
2 -13 -21 0.1834
2 21 -16 0.1343
-1 0 0 0.0360
1 0 0 0.0511
1 28 -4 0.0962
2 -17 -19 0.1694
19 -1 -2 0.0696
2 22 -15 0.1289
2 -19 -18 0.1626
0 28 -1 0.0888
-2 -19 17 0.1448
-2 19 18 0.1678
-18 3 10 0.0886

_exptl_crystal_size_max          0.418
_exptl_crystal_size_mid          0.185
_exptl_crystal_size_min          0.087
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-18.5694 0.4480 -0.8721 -1.0000 -0.0000 -0.0000
18.4146 -0.1303 2.0326 0.9988 0.0000 0.0499
-0.6520 -28.1163 2.9889 -0.0000 -0.9950 -0.0995
2.3033 -13.3583 -21.0545 -0.0000 -0.2617 -0.9651
2.0952 20.9377 -16.0705 0.0000 0.8710 -0.4913
-1.0028 -0.0035 -0.0086 -0.0537 -0.0013 0.0013
1.0028 0.0035 0.0086 0.0537 0.0013 -0.0013
0.7526 27.9638 -3.8685 0.0000 0.9981 0.0624
2.0693 -16.6108 -19.3453 -0.0000 -0.3896 -0.9210
18.7543 -1.2655 -2.1437 0.9916 -0.0000 -0.1293
1.9387 22.4181 -14.5867 0.0000 0.9080 -0.4191
1.8277 -19.2652 -17.5143 -0.0000 -0.4981 -0.8671
0.3658 28.3352 -0.5066 0.0000 0.9793 0.2026
-2.2361 -19.3413 17.4312 -0.0000 -0.8288 0.5595
-1.8650 18.8920 17.8001 0.0000 0.4826 0.8758
-17.5994 3.4050 10.2598 -0.8805 0.0000 0.4741

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1102
_diffrn_reflns_av_unetI/netI     0.1103
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            44991
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.604
_diffrn_reflns_theta_min         2.297
_diffrn_ambient_temperature      293.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -43.00 -17.50   0.50  418.85    --   20.00  54.00-153.20   51
  2  ω      5.00 109.50   0.50  418.85    --   20.00  54.00-153.20  209
  3  ω    -74.00 -44.50   0.50  418.85    --   20.00  54.00 120.00   59
  4  ω    -38.00  44.50   0.50  418.85    --   20.00  54.00 120.00  165
  5  ω     61.00  86.50   0.50  418.85    --   20.00  54.00 120.00   51
  6  ω    -73.00 -30.50   0.50  418.85    --   20.00  54.00   0.00   85
  7  ω     -7.00 107.50   0.50  418.85    --   20.00  54.00   0.00  229
  8  ω     45.00  81.50   0.50  418.85    --   20.00  54.00  26.80   73
  9  ω    -64.00 -27.50   0.50  418.85    --   20.00  54.00  30.00   73
 10  ω     60.00  84.50   0.50  418.85    --   20.00  54.00  30.00   49
 11  ω    -18.00   6.50   0.50  418.85    --   20.00  54.00  90.00   49
 12  ω     76.00 100.50   0.50  418.85    --   20.00  54.00  90.00   49
 13  ω    -69.00 -44.50   0.50  418.85    --   20.00  54.00-153.20   49
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II (JP)'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0535457000
_diffrn_orient_matrix_UB_12      -0.0005799000
_diffrn_orient_matrix_UB_13      0.0062256000
_diffrn_orient_matrix_UB_21      0.0012634000
_diffrn_orient_matrix_UB_22      0.0343783000
_diffrn_orient_matrix_UB_23      -0.0092423000
_diffrn_orient_matrix_UB_31      -0.0017182000
_diffrn_orient_matrix_UB_32      0.0078991000
_diffrn_orient_matrix_UB_33      0.0406404000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7369
_reflns_number_total             13167
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         13167
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1235
_refine_ls_R_factor_gt           0.0633
_refine_ls_restrained_S_all      0.975
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0761P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1511
_refine_ls_wR_factor_ref         0.1810
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00N(H00B,H00C), C012(H01A,H01B), C015(H01C,H01D), C018(H01E,H01F), C01B(H01H,
 H01I), C01G(H01O,H01P)
2.b Aromatic/amide H refined with riding coordinates:
 C00A(H00A), C00O(H00O), C00X(H00X), C00Y(H00Y), C00Z(H00Z), C011(H011),
 C013(H013), C016(H016), C01A(H01G), C01C(H01J), C01E(H01K), C01H(H01Q),
 C01I(H01R), C01K(H01V), C01L(H01W), C01M(H01X), C01O(H01Y), C01P(H01Z),
 C01Q(H01), C01S(H1), C01T(H2), C01U(H3)
2.c Idealised Me refined as rotating group:
 C01F(H01L,H01M,H01N), C01J(H01S,H01T,H01U), C01V(H4,H,HA), C01W(H5,HB,HC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S001 S 0.46003(5) 0.09567(3) 0.30492(4) 0.03889(16) Uani 1 1 d . . . . .
S002 S 0.26738(5) 0.26108(3) 0.53491(4) 0.04051(16) Uani 1 1 d . . . . .
O003 O 0.60811(12) 0.50632(7) 0.43194(9) 0.0350(4) Uani 1 1 d . . . . .
O004 O 0.83602(12) 0.15462(8) 0.61488(9) 0.0377(4) Uani 1 1 d . . . . .
O005 O 0.54553(14) 0.05130(8) 0.31399(10) 0.0476(4) Uani 1 1 d . . . . .
O006 O 0.39683(15) 0.09996(8) 0.23092(10) 0.0510(5) Uani 1 1 d . . . . .
O007 O 0.23901(14) 0.32887(8) 0.51568(12) 0.0567(5) Uani 1 1 d . . . . .
O008 O 0.25127(14) 0.21090(10) 0.47405(10) 0.0546(5) Uani 1 1 d . . . . .
N009 N 0.50408(15) 0.16938(8) 0.32465(11) 0.0372(5) Uani 1 1 d . . . . .
C00A C 0.77205(16) 0.22162(11) 0.50453(12) 0.0301(5) Uani 1 1 d . . . . .
H00A H 0.719217 0.191510 0.494298 0.036 Uiso 1 1 calc R U . . .
C00B C 0.76266(16) 0.41066(10) 0.38822(12) 0.0284(5) Uani 1 1 d . . . . .
C00C C 0.68216(15) 0.30031(10) 0.40508(11) 0.0256(4) Uani 1 1 d . . . . .
N10 N 0.38487(15) 0.26263(9) 0.57390(13) 0.0473(5) Uani 1 1 d . . . . .
C00E C 0.77261(15) 0.28035(10) 0.45846(11) 0.0273(4) Uani 1 1 d . . . . .
C00F C 0.60082(16) 0.25775(10) 0.37880(11) 0.0266(4) Uani 1 1 d . . . . .
C00G C 0.57208(16) 0.39491(10) 0.36227(12) 0.0279(4) Uani 1 1 d . . . . .
C00H C 0.67099(15) 0.36897(10) 0.38441(11) 0.0261(4) Uani 1 1 d . . . . .
C00I C 0.49224(16) 0.35219(10) 0.33666(12) 0.0286(5) Uani 1 1 d . . . . .
C00J C 0.75364(17) 0.42729(11) 0.64322(13) 0.0341(5) Uani 1 1 d . . . . .
C00K C 0.85418(16) 0.38848(11) 0.43134(12) 0.0299(5) Uani 1 1 d . . . . .
C00L C 0.84802(17) 0.20839(11) 0.56392(12) 0.0332(5) Uani 1 1 d . . . . .
C00M C 0.85540(16) 0.32491(10) 0.47347(12) 0.0293(5) Uani 1 1 d . . . . .
C00N C 0.54121(17) 0.46704(10) 0.37751(13) 0.0342(5) Uani 1 1 d . . . . .
H00B H 0.532745 0.489984 0.326795 0.041 Uiso 1 1 calc R U . . .
H00C H 0.475644 0.466054 0.397253 0.041 Uiso 1 1 calc R U . . .
C00O C 0.76381(17) 0.47061(11) 0.34495(13) 0.0336(5) Uani 1 1 d . . . . .
H00O H 0.705847 0.484087 0.313225 0.040 Uiso 1 1 calc R U . . .
C00P C 0.64215(16) 0.32671(10) 0.63195(12) 0.0295(5) Uani 1 1 d . . . . .
C00Q C 0.64772(17) 0.48058(10) 0.50428(13) 0.0317(5) Uani 1 1 d . . . . .
C00R C 0.55241(16) 0.29281(10) 0.60541(12) 0.0287(4) Uani 1 1 d . . . . .
C00S C 0.51169(16) 0.28332(10) 0.34021(12) 0.0277(4) Uani 1 1 d . . . . .
C00T C 0.62611(17) 0.18632(11) 0.65213(12) 0.0318(5) Uani 1 1 d . . . . .
C00U C 0.66674(16) 0.39466(10) 0.60654(13) 0.0308(5) Uani 1 1 d . . . . .
C00V C 0.20653(16) 0.23462(11) 0.61697(14) 0.0350(5) Uani 1 1 d . . . . .
C00W C 0.54401(16) 0.22476(10) 0.61993(12) 0.0309(5) Uani 1 1 d . . . . .
C00X C 0.73026(18) 0.51500(11) 0.54274(14) 0.0370(5) Uani 1 1 d . . . . .
H00X H 0.750844 0.555003 0.522199 0.044 Uiso 1 1 calc R U . . .
C00Y C 0.93760(18) 0.48974(12) 0.39409(14) 0.0420(6) Uani 1 1 d . . . . .
H00Y H 0.994719 0.516622 0.397489 0.050 Uiso 1 1 calc R U . . .
C00Z C 0.61375(16) 0.42331(10) 0.53810(13) 0.0302(5) Uani 1 1 d . . . . .
H00Z H 0.554620 0.403281 0.515155 0.036 Uiso 1 1 calc R U . . .
C010 C 0.71813(16) 0.29052(11) 0.68016(12) 0.0306(5) Uani 1 1 d . . . . .
C011 C 0.93534(17) 0.30686(12) 0.53164(13) 0.0394(6) Uani 1 1 d . . . . .
H011 H 0.992049 0.334035 0.539665 0.047 Uiso 1 1 calc R U . . .
C012 C 0.45321(16) 0.31842(10) 0.56240(13) 0.0324(5) Uani 1 1 d . . . . .
H01A H 0.431486 0.358954 0.586469 0.039 Uiso 1 1 calc R U . . .
H01B H 0.458481 0.326258 0.506481 0.039 Uiso 1 1 calc R U . . .
C013 C 0.78068(18) 0.48930(11) 0.61106(14) 0.0390(6) Uani 1 1 d . . . . .
H013 H 0.834267 0.513161 0.637215 0.047 Uiso 1 1 calc R U . . .
C014 C 0.71513(17) 0.21908(11) 0.68064(12) 0.0322(5) Uani 1 1 d . . . . .
C015 C 0.43819(17) 0.22858(10) 0.31234(13) 0.0335(5) Uani 1 1 d . . . . .
H01C H 0.382239 0.226531 0.344301 0.040 Uiso 1 1 calc R U . . .
H01D H 0.412207 0.234005 0.256854 0.040 Uiso 1 1 calc R U . . .
C016 C 0.84983(19) 0.50970(12) 0.34895(14) 0.0407(6) Uani 1 1 d . . . . .
H016 H 0.848534 0.549616 0.321110 0.049 Uiso 1 1 calc R U . . .
C017 C 0.37920(19) 0.07181(11) 0.37680(14) 0.0393(6) Uani 1 1 d . . . . .
C018 C 0.59338(17) 0.18190(10) 0.38260(13) 0.0327(5) Uani 1 1 d . . . . .
H01E H 0.653313 0.160705 0.366635 0.039 Uiso 1 1 calc R U . . .
H01F H 0.582595 0.166829 0.435408 0.039 Uiso 1 1 calc R U . . .
C019 C 0.79718(17) 0.32848(11) 0.72837(13) 0.0339(5) Uani 1 1 d . . . . .
C01A C 0.17288(19) 0.16931(11) 0.62138(16) 0.0434(6) Uani 1 1 d . . . . .
H01G H 0.178474 0.139811 0.579797 0.052 Uiso 1 1 calc R U . . .
C01B C 0.43976(17) 0.19989(11) 0.59061(14) 0.0370(5) Uani 1 1 d . . . . .
H01H H 0.440226 0.173108 0.542995 0.044 Uiso 1 1 calc R U . . .
H01I H 0.411078 0.174188 0.631057 0.044 Uiso 1 1 calc R U . . .
C01C C 0.94033(17) 0.42995(12) 0.43404(13) 0.0373(5) Uani 1 1 d . . . . .
H01J H 1.000090 0.416547 0.463419 0.045 Uiso 1 1 calc R U . . .
C01D C 0.81416(18) 0.39644(12) 0.71055(13) 0.0379(5) Uani 1 1 d . . . . .
C01E C 0.93141(18) 0.24990(12) 0.57687(13) 0.0402(6) Uani 1 1 d . . . . .
H01K H 0.984189 0.239492 0.615623 0.048 Uiso 1 1 calc R U . . .
C01F C 0.38735(17) 0.37659(11) 0.30796(15) 0.0419(6) Uani 1 1 d . . . . .
H01L H 0.351574 0.385965 0.352835 0.063 Uiso 1 1 calc R U . . .
H01M H 0.351890 0.342979 0.275614 0.063 Uiso 1 1 calc R U . . .
H01N H 0.391862 0.416337 0.277152 0.063 Uiso 1 1 calc R U . . .
C01G C 0.81273(18) 0.17845(12) 0.69271(13) 0.0384(6) Uani 1 1 d . . . . .
H01O H 0.867610 0.205863 0.717088 0.046 Uiso 1 1 calc R U . . .
H01P H 0.804397 0.141014 0.727511 0.046 Uiso 1 1 calc R U . . .
C01H C 0.84915(18) 0.30107(13) 0.79830(13) 0.0420(6) Uani 1 1 d . . . . .
H01Q H 0.834193 0.257897 0.812799 0.050 Uiso 1 1 calc R U . . .
C01I C 0.4189(2) 0.05824(12) 0.45431(15) 0.0460(6) Uani 1 1 d . . . . .
H01R H 0.486989 0.065948 0.470441 0.055 Uiso 1 1 calc R U . . .
C01J C 0.61678(19) 0.11098(11) 0.65042(14) 0.0411(6) Uani 1 1 d . . . . .
H01S H 0.547654 0.098651 0.653179 0.062 Uiso 1 1 calc R U . . .
H01T H 0.658361 0.092438 0.695004 0.062 Uiso 1 1 calc R U . . .
H01U H 0.638426 0.094272 0.601984 0.062 Uiso 1 1 calc R U . . .
C01K C 0.8897(2) 0.43105(14) 0.75944(16) 0.0523(7) Uani 1 1 d . . . . .
H01V H 0.903950 0.474877 0.747225 0.063 Uiso 1 1 calc R U . . .
C01L C 0.9213(2) 0.33648(15) 0.84556(15) 0.0517(7) Uani 1 1 d . . . . .
H01W H 0.955276 0.317158 0.890813 0.062 Uiso 1 1 calc R U . . .
C01M C 0.1307(2) 0.14879(14) 0.68903(18) 0.0539(7) Uani 1 1 d . . . . .
H01X H 0.107554 0.105310 0.691824 0.065 Uiso 1 1 calc R U . . .
C01N C 0.12233(19) 0.19119(16) 0.75183(16) 0.0535(7) Uani 1 1 d . . . . .
C01O C 0.19851(19) 0.27840(13) 0.67939(16) 0.0484(6) Uani 1 1 d . . . . .
H01Y H 0.221197 0.321963 0.676458 0.058 Uiso 1 1 calc R U . . .
C01P C 0.3568(2) 0.03305(13) 0.50795(17) 0.0564(7) Uani 1 1 d . . . . .
H01Z H 0.383757 0.025102 0.560171 0.068 Uiso 1 1 calc R U . . .
C01Q C 0.9427(2) 0.40157(16) 0.82477(16) 0.0605(8) Uani 1 1 d . . . . .
H01 H 0.993072 0.425259 0.855183 0.073 Uiso 1 1 calc R U . . .
C01R C 0.2572(3) 0.01974(15) 0.4858(2) 0.0642(8) Uani 1 1 d . . . . .
C01S C 0.2773(2) 0.06129(14) 0.35412(19) 0.0617(8) Uani 1 1 d . . . . .
H1 H 0.248894 0.072206 0.303064 0.074 Uiso 1 1 calc R U . . .
C01T C 0.1564(2) 0.25670(15) 0.74622(17) 0.0563(7) Uani 1 1 d . . . . .
H2 H 0.150698 0.286119 0.787864 0.068 Uiso 1 1 calc R U . . .
C01U C 0.2180(2) 0.03430(17) 0.4084(2) 0.0773(10) Uani 1 1 d . . . . .
H3 H 0.150167 0.025751 0.392369 0.093 Uiso 1 1 calc R U . . .
C01V C 0.0795(3) 0.16809(19) 0.82583(18) 0.0835(12) Uani 1 1 d . . . . .
H4 H 0.031604 0.133093 0.812435 0.125 Uiso 1 1 calc R U . . .
H H 0.046481 0.204607 0.848723 0.125 Uiso 1 1 calc R U . . .
HA H 0.133186 0.151851 0.863479 0.125 Uiso 1 1 calc R U . . .
C01W C 0.1907(3) -0.01290(18) 0.5427(2) 0.1041(15) Uani 1 1 d . . . . .
H5 H 0.178110 -0.058349 0.527272 0.156 Uiso 1 1 calc R U . . .
HB H 0.127660 0.010559 0.540635 0.156 Uiso 1 1 calc R U . . .
HC H 0.224373 -0.011398 0.595833 0.156 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S001 O005 1.4417(18) . ?
S001 O006 1.4312(16) . ?
S001 N009 1.6155(18) . ?
S001 C017 1.779(3) . ?
S002 O007 1.4423(17) . ?
S002 O008 1.4409(18) . ?
S002 N10 1.629(2) . ?
S002 C00V 1.767(2) . ?
O003 C00N 1.443(2) . ?
O003 C00Q 1.379(3) . ?
O004 C00L 1.404(3) . ?
O004 C01G 1.468(3) . ?
N009 C015 1.480(3) . ?
N009 C018 1.476(3) . ?
C00A H00A 0.9300 . ?
C00A C00E 1.416(3) . ?
C00A C00L 1.370(3) . ?
C00B C00H 1.477(3) . ?
C00B C00K 1.421(3) . ?
C00B C00O 1.412(3) . ?
C00C C00E 1.478(3) . ?
C00C C00F 1.413(3) . ?
C00C C00H 1.428(3) . ?
N10 C012 1.472(3) . ?
N10 C01B 1.470(3) . ?
C00E C00M 1.422(3) . ?
C00F C00S 1.388(3) . ?
C00F C018 1.530(3) . ?
C00G C00H 1.428(3) . ?
C00G C00I 1.398(3) . ?
C00G C00N 1.538(3) . ?
C00I C00S 1.409(3) . ?
C00I C01F 1.509(3) . ?
C00J C00U 1.412(3) . ?
C00J C013 1.423(3) . ?
C00J C01D 1.459(3) . ?
C00K C00M 1.463(3) . ?
C00K C01C 1.415(3) . ?
C00L C01E 1.387(3) . ?
C00M C011 1.414(3) . ?
C00N H00B 0.9700 . ?
C00N H00C 0.9700 . ?
C00O H00O 0.9300 . ?
C00O C016 1.385(3) . ?
C00P C00R 1.405(3) . ?
C00P C00U 1.480(3) . ?
C00P C010 1.426(3) . ?
C00Q C00X 1.397(3) . ?
C00Q C00Z 1.385(3) . ?
C00R C00W 1.397(3) . ?
C00R C012 1.525(3) . ?
C00S C015 1.513(3) . ?
C00T C00W 1.399(3) . ?
C00T C014 1.395(3) . ?
C00T C01J 1.520(3) . ?
C00U C00Z 1.410(3) . ?
C00V C01A 1.393(3) . ?
C00V C01O 1.389(3) . ?
C00W C01B 1.507(3) . ?
C00X H00X 0.9300 . ?
C00X C013 1.372(3) . ?
C00Y H00Y 0.9300 . ?
C00Y C016 1.383(3) . ?
C00Y C01C 1.378(3) . ?
C00Z H00Z 0.9300 . ?
C010 C014 1.437(3) . ?
C010 C019 1.471(3) . ?
C011 H011 0.9300 . ?
C011 C01E 1.382(3) . ?
C012 H01A 0.9700 . ?
C012 H01B 0.9700 . ?
C013 H013 0.9300 . ?
C014 C01G 1.530(3) . ?
C015 H01C 0.9700 . ?
C015 H01D 0.9700 . ?
C016 H016 0.9300 . ?
C017 C01I 1.386(3) . ?
C017 C01S 1.385(4) . ?
C018 H01E 0.9700 . ?
C018 H01F 0.9700 . ?
C019 C01D 1.423(3) . ?
C019 C01H 1.414(3) . ?
C01A H01G 0.9300 . ?
C01A C01M 1.394(4) . ?
C01B H01H 0.9700 . ?
C01B H01I 0.9700 . ?
C01C H01J 0.9300 . ?
C01D C01K 1.412(3) . ?
C01E H01K 0.9300 . ?
C01F H01L 0.9600 . ?
C01F H01M 0.9600 . ?
C01F H01N 0.9600 . ?
C01G H01O 0.9700 . ?
C01G H01P 0.9700 . ?
C01H H01Q 0.9300 . ?
C01H C01L 1.377(3) . ?
C01I H01R 0.9300 . ?
C01I C01P 1.392(4) . ?
C01J H01S 0.9600 . ?
C01J H01T 0.9600 . ?
C01J H01U 0.9600 . ?
C01K H01V 0.9300 . ?
C01K C01Q 1.378(4) . ?
C01L H01W 0.9300 . ?
C01L C01Q 1.393(4) . ?
C01M H01X 0.9300 . ?
C01M C01N 1.377(4) . ?
C01N C01T 1.400(4) . ?
C01N C01V 1.507(4) . ?
C01O H01Y 0.9300 . ?
C01O C01T 1.389(4) . ?
C01P H01Z 0.9300 . ?
C01P C01R 1.363(4) . ?
C01Q H01 0.9300 . ?
C01R C01U 1.387(4) . ?
C01R C01W 1.529(4) . ?
C01S H1 0.9300 . ?
C01S C01U 1.387(4) . ?
C01T H2 0.9300 . ?
C01U H3 0.9300 . ?
C01V H4 0.9600 . ?
C01V H 0.9600 . ?
C01V HA 0.9600 . ?
C01W H5 0.9600 . ?
C01W HB 0.9600 . ?
C01W HC 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O005 S001 N009 106.36(10) . . ?
O005 S001 C017 106.98(11) . . ?
O006 S001 O005 120.71(11) . . ?
O006 S001 N009 106.86(10) . . ?
O006 S001 C017 105.85(11) . . ?
N009 S001 C017 109.86(11) . . ?
O007 S002 N10 106.79(10) . . ?
O007 S002 C00V 109.29(11) . . ?
O008 S002 O007 119.10(12) . . ?
O008 S002 N10 111.23(11) . . ?
O008 S002 C00V 107.86(11) . . ?
N10 S002 C00V 101.08(11) . . ?
C00Q O003 C00N 120.59(16) . . ?
C00L O004 C01G 110.52(17) . . ?
C015 N009 S001 120.87(15) . . ?
C018 N009 S001 122.75(14) . . ?
C018 N009 C015 112.17(16) . . ?
C00E C00A H00A 119.4 . . ?
C00L C00A H00A 119.4 . . ?
C00L C00A C00E 121.1(2) . . ?
C00K C00B C00H 120.14(18) . . ?
C00O C00B C00H 121.29(19) . . ?
C00O C00B C00K 118.42(19) . . ?
C00F C00C C00E 124.86(18) . . ?
C00F C00C C00H 116.96(18) . . ?
C00H C00C C00E 117.89(18) . . ?
C012 N10 S002 122.79(15) . . ?
C01B N10 S002 119.74(16) . . ?
C01B N10 C012 112.21(18) . . ?
C00A C00E C00C 120.59(18) . . ?
C00A C00E C00M 118.64(18) . . ?
C00M C00E C00C 120.06(19) . . ?
C00C C00F C018 129.91(18) . . ?
C00S C00F C00C 120.60(19) . . ?
C00S C00F C018 109.45(18) . . ?
C00H C00G C00N 123.86(18) . . ?
C00I C00G C00H 120.31(18) . . ?
C00I C00G C00N 115.04(18) . . ?
C00C C00H C00B 118.37(18) . . ?
C00G C00H C00B 122.58(18) . . ?
C00G C00H C00C 119.03(18) . . ?
C00G C00I C00S 117.45(19) . . ?
C00G C00I C01F 123.03(19) . . ?
C00S C00I C01F 119.50(19) . . ?
C00U C00J C013 118.0(2) . . ?
C00U C00J C01D 120.0(2) . . ?
C013 C00J C01D 122.0(2) . . ?
C00B C00K C00M 119.12(19) . . ?
C01C C00K C00B 118.5(2) . . ?
C01C C00K C00M 122.3(2) . . ?
C00A C00L O004 118.4(2) . . ?
C00A C00L C01E 120.8(2) . . ?
C01E C00L O004 120.73(19) . . ?
C00E C00M C00K 119.85(19) . . ?
C011 C00M C00E 118.1(2) . . ?
C011 C00M C00K 122.0(2) . . ?
O003 C00N C00G 117.76(18) . . ?
O003 C00N H00B 107.9 . . ?
O003 C00N H00C 107.9 . . ?
C00G C00N H00B 107.9 . . ?
C00G C00N H00C 107.9 . . ?
H00B C00N H00C 107.2 . . ?
C00B C00O H00O 119.5 . . ?
C016 C00O C00B 121.1(2) . . ?
C016 C00O H00O 119.5 . . ?
C00R C00P C00U 124.3(2) . . ?
C00R C00P C010 117.31(19) . . ?
C010 C00P C00U 118.11(19) . . ?
O003 C00Q C00X 115.50(19) . . ?
O003 C00Q C00Z 124.7(2) . . ?
C00Z C00Q C00X 119.8(2) . . ?
C00P C00R C012 130.48(19) . . ?
C00W C00R C00P 120.07(19) . . ?
C00W C00R C012 109.42(18) . . ?
C00F C00S C00I 121.85(18) . . ?
C00F C00S C015 111.51(18) . . ?
C00I C00S C015 126.32(19) . . ?
C00W C00T C01J 119.0(2) . . ?
C014 C00T C00W 118.1(2) . . ?
C014 C00T C01J 122.8(2) . . ?
C00J C00U C00P 119.9(2) . . ?
C00Z C00U C00J 118.8(2) . . ?
C00Z C00U C00P 120.60(19) . . ?
C01A C00V S002 120.34(19) . . ?
C01O C00V S002 119.25(19) . . ?
C01O C00V C01A 120.3(2) . . ?
C00R C00W C00T 122.4(2) . . ?
C00R C00W C01B 110.88(18) . . ?
C00T C00W C01B 126.60(19) . . ?
C00Q C00X H00X 120.3 . . ?
C013 C00X C00Q 119.4(2) . . ?
C013 C00X H00X 120.3 . . ?
C016 C00Y H00Y 120.0 . . ?
C01C C00Y H00Y 120.0 . . ?
C01C C00Y C016 119.9(2) . . ?
C00Q C00Z C00U 121.5(2) . . ?
C00Q C00Z H00Z 119.2 . . ?
C00U C00Z H00Z 119.2 . . ?
C00P C010 C014 119.66(19) . . ?
C00P C010 C019 118.06(19) . . ?
C014 C010 C019 122.3(2) . . ?
C00M C011 H011 119.1 . . ?
C01E C011 C00M 121.7(2) . . ?
C01E C011 H011 119.1 . . ?
N10 C012 C00R 101.26(17) . . ?
N10 C012 H01A 111.5 . . ?
N10 C012 H01B 111.5 . . ?
C00R C012 H01A 111.5 . . ?
C00R C012 H01B 111.5 . . ?
H01A C012 H01B 109.3 . . ?
C00J C013 H013 118.9 . . ?
C00X C013 C00J 122.1(2) . . ?
C00X C013 H013 118.9 . . ?
C00T C014 C010 119.56(19) . . ?
C00T C014 C01G 118.1(2) . . ?
C010 C014 C01G 120.7(2) . . ?
N009 C015 C00S 100.86(17) . . ?
N009 C015 H01C 111.6 . . ?
N009 C015 H01D 111.6 . . ?
C00S C015 H01C 111.6 . . ?
C00S C015 H01D 111.6 . . ?
H01C C015 H01D 109.4 . . ?
C00O C016 H016 119.8 . . ?
C00Y C016 C00O 120.4(2) . . ?
C00Y C016 H016 119.8 . . ?
C01I C017 S001 120.30(19) . . ?
C01S C017 S001 120.1(2) . . ?
C01S C017 C01I 119.4(3) . . ?
N009 C018 C00F 101.14(16) . . ?
N009 C018 H01E 111.5 . . ?
N009 C018 H01F 111.5 . . ?
C00F C018 H01E 111.5 . . ?
C00F C018 H01F 111.5 . . ?
H01E C018 H01F 109.4 . . ?
C01D C019 C010 120.1(2) . . ?
C01H C019 C010 121.0(2) . . ?
C01H C019 C01D 118.5(2) . . ?
C00V C01A H01G 120.5 . . ?
C00V C01A C01M 119.0(3) . . ?
C01M C01A H01G 120.5 . . ?
N10 C01B C00W 101.46(17) . . ?
N10 C01B H01H 111.5 . . ?
N10 C01B H01I 111.5 . . ?
C00W C01B H01H 111.5 . . ?
C00W C01B H01I 111.5 . . ?
H01H C01B H01I 109.3 . . ?
C00K C01C H01J 119.3 . . ?
C00Y C01C C00K 121.5(2) . . ?
C00Y C01C H01J 119.3 . . ?
C019 C01D C00J 119.1(2) . . ?
C01K C01D C00J 122.9(2) . . ?
C01K C01D C019 118.0(2) . . ?
C00L C01E H01K 120.3 . . ?
C011 C01E C00L 119.4(2) . . ?
C011 C01E H01K 120.3 . . ?
C00I C01F H01L 109.5 . . ?
C00I C01F H01M 109.5 . . ?
C00I C01F H01N 109.5 . . ?
H01L C01F H01M 109.5 . . ?
H01L C01F H01N 109.5 . . ?
H01M C01F H01N 109.5 . . ?
O004 C01G C014 108.47(16) . . ?
O004 C01G H01O 110.0 . . ?
O004 C01G H01P 110.0 . . ?
C014 C01G H01O 110.0 . . ?
C014 C01G H01P 110.0 . . ?
H01O C01G H01P 108.4 . . ?
C019 C01H H01Q 119.0 . . ?
C01L C01H C019 121.9(2) . . ?
C01L C01H H01Q 119.0 . . ?
C017 C01I H01R 120.1 . . ?
C017 C01I C01P 119.8(3) . . ?
C01P C01I H01R 120.1 . . ?
C00T C01J H01S 109.5 . . ?
C00T C01J H01T 109.5 . . ?
C00T C01J H01U 109.5 . . ?
H01S C01J H01T 109.5 . . ?
H01S C01J H01U 109.5 . . ?
H01T C01J H01U 109.5 . . ?
C01D C01K H01V 119.1 . . ?
C01Q C01K C01D 121.7(3) . . ?
C01Q C01K H01V 119.1 . . ?
C01H C01L H01W 120.4 . . ?
C01H C01L C01Q 119.2(2) . . ?
C01Q C01L H01W 120.4 . . ?
C01A C01M H01X 119.1 . . ?
C01N C01M C01A 121.7(3) . . ?
C01N C01M H01X 119.1 . . ?
C01M C01N C01T 118.4(3) . . ?
C01M C01N C01V 121.5(3) . . ?
C01T C01N C01V 120.1(3) . . ?
C00V C01O H01Y 120.2 . . ?
C01T C01O C00V 119.6(3) . . ?
C01T C01O H01Y 120.2 . . ?
C01I C01P H01Z 119.2 . . ?
C01R C01P C01I 121.6(3) . . ?
C01R C01P H01Z 119.2 . . ?
C01K C01Q C01L 120.4(3) . . ?
C01K C01Q H01 119.8 . . ?
C01L C01Q H01 119.8 . . ?
C01P C01R C01U 118.0(3) . . ?
C01P C01R C01W 121.8(3) . . ?
C01U C01R C01W 120.2(3) . . ?
C017 C01S H1 120.3 . . ?
C017 C01S C01U 119.3(3) . . ?
C01U C01S H1 120.3 . . ?
C01N C01T H2 119.5 . . ?
C01O C01T C01N 121.0(3) . . ?
C01O C01T H2 119.5 . . ?
C01R C01U C01S 121.8(3) . . ?
C01R C01U H3 119.1 . . ?
C01S C01U H3 119.1 . . ?
C01N C01V H4 109.5 . . ?
C01N C01V H 109.5 . . ?
C01N C01V HA 109.5 . . ?
H4 C01V H 109.5 . . ?
H4 C01V HA 109.5 . . ?
H C01V HA 109.5 . . ?
C01R C01W H5 109.5 . . ?
C01R C01W HB 109.5 . . ?
C01R C01W HC 109.5 . . ?
H5 C01W HB 109.5 . . ?
H5 C01W HC 109.5 . . ?
HB C01W HC 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.400
_oxdiff_exptl_absorpt_empirical_full_min 0.723
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_529_auto
_database_code_depnum_ccdc_archive 'CCDC 2237886'
loop_
_audit_author_name
_audit_author_address
'Juntaro Nogami'
;Tokyo Institute of Technology
Japan
;
_audit_update_record             
;
2023-01-25 deposited with the CCDC.	2023-03-10 downloaded from the CCDC.
;
_audit_creation_date             2023-01-23
_audit_creation_method           
;
Olex2 1.5-ac5-023
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            (+-)-3e
_chemical_name_systematic        '[2.2][5]Helicenophane'
_chemical_formula_moiety         'C70 H52 O2'
_chemical_formula_sum            'C70 H52 O2'
_chemical_formula_weight         925.11
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.9227(4)
_cell_length_b                   24.0368(7)
_cell_length_c                   17.1320(5)
_cell_angle_alpha                90
_cell_angle_beta                 97.506(3)
_cell_angle_gamma                90
_cell_volume                     5275.9(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    12231
_cell_measurement_temperature    210
_cell_measurement_theta_max      28.0240
_cell_measurement_theta_min      2.0780
_shelx_estimated_absorpt_T_max   0.988
_shelx_estimated_absorpt_T_min   0.977
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.973
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.61a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1952
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 10 22 0.1358
-5 -29 -9 0.0721
-1 -16 21 0.1684
17 -11 -3 0.0691
5 32 -5 0.1092
3 13 21 0.1303
5 31 7 0.1184
17 -3 -13 0.0993
-2 -15 22 0.1710
-2 -14 22 0.1712
-5 -29 -10 0.0660
-16 14 -3 0.0759
3 -17 20 0.1674
17 -11 -2 0.0722
-17 5 10 0.1262
4 14 -22 0.1690
16 0 -15 0.1082

_exptl_crystal_size_max          0.345
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.172
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
2.4107 10.3763 22.1591 -0.0000 -0.7288 -0.6847
-5.1705 -29.1667 -9.2394 0.0000 0.9991 -0.0416
-0.6599 -15.9215 21.2319 0.0712 0.0000 -0.9975
17.2871 -10.7030 -2.9495 0.9991 0.0000 -0.0434
5.2101 31.9643 -4.9497 -0.0000 -0.7967 0.6044
2.8068 12.8831 21.3556 -0.0000 -0.7831 -0.6219
5.3259 30.5428 6.7491 -0.0000 -0.9884 0.1521
16.5600 -2.6609 -12.6439 0.9062 -0.0000 0.4229
-2.2081 -15.0655 21.6288 -0.0175 0.0000 -0.9998
-1.6330 -13.7222 22.0673 -0.0000 -0.0526 -0.9986
-5.0957 -28.5568 -10.1460 0.0000 1.0000 0.0000
-15.8921 14.3552 -3.1289 -0.9487 -0.0000 0.3162
2.5207 -17.2786 19.8975 0.2510 -0.0000 -0.9680
17.1681 -11.2816 -2.0856 0.9965 -0.0000 -0.0830
-17.1232 4.8465 10.3644 -0.9510 0.0000 -0.3091
3.7448 14.0867 -21.8555 0.1065 -0.0000 0.9943
15.5221 0.0936 -15.1980 0.8321 0.0000 0.5547

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0992
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            55196
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.653
_diffrn_reflns_theta_min         2.324
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      210
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     85.00 110.00   0.50   84.92    --   20.00  54.00 -30.00   50
  2  ω    -70.00 -15.00   0.50   84.92    --   20.00  54.00 120.00  110
  3  ω     43.00  72.00   0.50   84.92    --   20.00  54.00 120.00   58
  4  ω     76.00 109.00   0.50   84.92    --   20.00  54.00 120.00   66
  5  ω    -74.00 107.00   0.50   84.92    --   20.00  54.00-120.00  362
  6  ω    -42.00   6.00   0.50   84.92    --   20.00  54.00-150.00   96
  7  ω     18.00  43.00   0.50   84.92    --   20.00  54.00-150.00   50
  8  ω     70.00  97.00   0.50   84.92    --   20.00  54.00-150.00   54
  9  ω    -17.00  83.00   0.50   84.92    --   20.00  54.00-180.00  200
 10  ω     11.00  36.00   0.50   84.92    --   20.00  54.00  60.00   50
 11  ω     75.00 100.00   0.50   84.92    --   20.00  54.00  60.00   50
 12  ω    -62.00 -33.00   0.50   84.92    --   20.00  54.00 -30.00   58
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II (JP)'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0521125000
_diffrn_orient_matrix_UB_12      -0.0087385000
_diffrn_orient_matrix_UB_13      -0.0015775000
_diffrn_orient_matrix_UB_21      -0.0186695000
_diffrn_orient_matrix_UB_22      -0.0248576000
_diffrn_orient_matrix_UB_23      -0.0192206000
_diffrn_orient_matrix_UB_31      -0.0006162000
_diffrn_orient_matrix_UB_32      0.0132720000
_diffrn_orient_matrix_UB_33      -0.0370459000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7720
_reflns_number_total             15579
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     671
_refine_ls_number_reflns         15579
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1502
_refine_ls_R_factor_gt           0.0765
_refine_ls_restrained_S_all      0.988
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0931P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1708
_refine_ls_wR_factor_ref         0.1958
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 C70-C71 \\sim C70-C71A
 with sigma of 0.02
 C70-C34 \\sim C70-C34A
 with sigma of 0.04
 C71-C34 \\sim C71A-C34A
 with sigma of 0.02
2. Others
 Sof(H70C)=Sof(H70D)=Sof(C71A)=Sof(H71C)=Sof(H71D)=Sof(C34A)=Sof(H34D)=
 Sof(H34E)=Sof(H34F)=1-FVAR(1)
 Sof(H70A)=Sof(H70B)=Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(C34)=Sof(H34A)=Sof(H34B)=
 Sof(H34C)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C61(H61A,H61B), C35(H35A,H35B), C33(H33A,H33B), C69(H69A,H69B), C62(H62A,
 H62B), C63(H63A,H63B), C70(H70A,H70B), C70(H70C,H70D), C71(H71A,H71B),
 C71A(H71C,H71D)
3.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C39(H39), C10(H10), C28(H28), C18(H18), C40(H40), C17(H17),
 C21(H21), C7(H7), C24(H24), C59(H59), C9(H9), C23(H23), C46(H46), C8(H8),
 C43(H43), C65(H65), C22(H22), C44(H44), C68(H68), C57(H57), C45(H45), C58(H58),
  C56(H56), C50(H50), C66(H66), C67(H67), C53(H53), C51(H51), C52(H52)
3.c Idealised Me refined as rotating group:
 C64(H64A,H64B,H64C), C34(H34A,H34B,H34C), C34A(H34D,H34E,H34F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O36 O 0.53508(12) 0.95398(5) 0.44196(8) 0.0341(4) Uani 1 1 d . . . . .
O34 O 0.77652(12) 0.69001(6) 0.32159(9) 0.0407(4) Uani 1 1 d . . . . .
C11 C 0.50641(17) 0.69266(8) 0.51813(11) 0.0286(5) Uani 1 1 d . . . . .
C6 C 0.41934(17) 0.65605(9) 0.50544(12) 0.0312(5) Uani 1 1 d . . . . .
C2 C 0.37412(16) 0.83316(9) 0.48549(11) 0.0302(5) Uani 1 1 d . . . . .
C12 C 0.49100(16) 0.75261(8) 0.50740(11) 0.0280(5) Uani 1 1 d . . . . .
C13 C 0.57723(16) 0.79051(8) 0.50410(11) 0.0261(4) Uani 1 1 d . . . . .
C30 C 0.54568(16) 0.80298(8) 0.25000(11) 0.0273(5) Uani 1 1 d . . . . .
C15 C 0.68186(17) 0.73424(8) 0.41924(12) 0.0307(5) Uani 1 1 d . . . . .
H15 H 0.624047 0.709912 0.407132 0.037 Uiso 1 1 calc R U . . .
C29 C 0.58786(16) 0.85537(8) 0.28536(11) 0.0278(5) Uani 1 1 d . . . . .
C14 C 0.67697(16) 0.77679(8) 0.47487(11) 0.0275(5) Uani 1 1 d . . . . .
C5 C 0.31468(18) 0.67897(9) 0.50126(12) 0.0361(5) Uani 1 1 d . . . . .
C1 C 0.45947(17) 0.86887(8) 0.49716(12) 0.0298(5) Uani 1 1 d . . . . .
C38 C 0.43784(16) 0.78772(9) 0.23946(12) 0.0301(5) Uani 1 1 d . . . . .
C26 C 0.56194(16) 0.84728(8) 0.51845(11) 0.0271(5) Uani 1 1 d . . . . .
C42 C 0.75132(17) 0.83673(10) 0.23087(12) 0.0341(5) Uani 1 1 d . . . . .
C3 C 0.38938(16) 0.77500(9) 0.50347(11) 0.0296(5) Uani 1 1 d . . . . .
C19 C 0.76324(17) 0.81274(9) 0.49174(12) 0.0314(5) Uani 1 1 d . . . . .
C25 C 0.65292(18) 0.88012(8) 0.54974(11) 0.0303(5) Uani 1 1 d . . . . .
C16 C 0.76928(18) 0.72724(9) 0.38195(12) 0.0352(5) Uani 1 1 d . . . . .
C27 C 0.57966(17) 0.92709(8) 0.38356(12) 0.0302(5) Uani 1 1 d . . . . .
C20 C 0.75394(17) 0.86104(8) 0.54169(12) 0.0325(5) Uani 1 1 d . . . . .
C31 C 0.61996(16) 0.76205(9) 0.23907(11) 0.0292(5) Uani 1 1 d . . . . .
C48 C 0.49183(17) 0.69069(9) 0.26182(12) 0.0314(5) Uani 1 1 d . . . . .
C39 C 0.67987(18) 0.94494(9) 0.37364(13) 0.0360(5) Uani 1 1 d . . . . .
H39 H 0.710481 0.975818 0.402614 0.043 Uiso 1 1 calc R U . . .
C47 C 0.72026(17) 0.78102(9) 0.21747(12) 0.0328(5) Uani 1 1 d . . . . .
C10 C 0.60457(18) 0.66939(9) 0.54413(13) 0.0358(5) Uani 1 1 d . . . . .
H10 H 0.662222 0.693417 0.558758 0.043 Uiso 1 1 calc R U . . .
C32 C 0.59438(17) 0.70561(9) 0.25471(12) 0.0314(5) Uani 1 1 d . . . . .
C28 C 0.53366(16) 0.88391(8) 0.33936(11) 0.0289(5) Uani 1 1 d . . . . .
H28 H 0.464372 0.873144 0.345255 0.035 Uiso 1 1 calc R U . . .
C18 C 0.85366(18) 0.80239(9) 0.45604(14) 0.0391(6) Uani 1 1 d . . . . .
H18 H 0.913630 0.824989 0.469594 0.047 Uiso 1 1 calc R U . . .
C41 C 0.69004(17) 0.87152(9) 0.27793(12) 0.0316(5) Uani 1 1 d . . . . .
C4 C 0.30232(17) 0.73706(9) 0.51107(12) 0.0342(5) Uani 1 1 d . . . . .
C40 C 0.73381(18) 0.91725(9) 0.32134(13) 0.0372(5) Uani 1 1 d . . . . .
H40 H 0.802038 0.929326 0.314475 0.045 Uiso 1 1 calc R U . . .
C17 C 0.85695(17) 0.76047(10) 0.40225(13) 0.0387(5) Uani 1 1 d . . . . .
H17 H 0.918675 0.754109 0.378927 0.046 Uiso 1 1 calc R U . . .
C60 C 0.35564(16) 0.83033(9) 0.22489(12) 0.0313(5) Uani 1 1 d . . . . .
C21 C 0.84065(19) 0.88930(10) 0.58100(13) 0.0417(6) Uani 1 1 d . . . . .
H21 H 0.908953 0.876099 0.576648 0.050 Uiso 1 1 calc R U . . .
C7 C 0.43788(19) 0.59813(9) 0.50907(12) 0.0387(6) Uani 1 1 d . . . . .
H7 H 0.380668 0.573343 0.497526 0.046 Uiso 1 1 calc R U . . .
C55 C 0.25270(17) 0.81684(10) 0.23587(13) 0.0380(5) Uani 1 1 d . . . . .
C24 C 0.64288(19) 0.92840(9) 0.59515(12) 0.0372(5) Uani 1 1 d . . . . .
H24 H 0.575265 0.942433 0.599918 0.045 Uiso 1 1 calc R U . . .
C37 C 0.41067(17) 0.73117(8) 0.24197(12) 0.0309(5) Uani 1 1 d . . . . .
C61 C 0.46885(18) 0.63579(8) 0.30064(12) 0.0356(5) Uani 1 1 d . . . . .
H61A H 0.396206 0.637289 0.313069 0.043 Uiso 1 1 calc R U . . .
H61B H 0.515165 0.633224 0.351317 0.043 Uiso 1 1 calc R U . . .
C59 C 0.37562(18) 0.88389(9) 0.19828(12) 0.0364(5) Uani 1 1 d . . . . .
H59 H 0.443024 0.892144 0.184918 0.044 Uiso 1 1 calc R U . . .
C35 C 0.44535(18) 0.92901(8) 0.46974(13) 0.0352(5) Uani 1 1 d . . . . .
H35A H 0.386103 0.930639 0.426874 0.042 Uiso 1 1 calc R U . . .
H35B H 0.426245 0.951609 0.514002 0.042 Uiso 1 1 calc R U . . .
C9 C 0.6196(2) 0.61249(9) 0.54904(14) 0.0433(6) Uani 1 1 d . . . . .
H9 H 0.687005 0.597801 0.566219 0.052 Uiso 1 1 calc R U . . .
C23 C 0.7295(2) 0.95556(10) 0.63270(13) 0.0437(6) Uani 1 1 d . . . . .
H23 H 0.721227 0.987805 0.663359 0.052 Uiso 1 1 calc R U . . .
C33 C 0.68310(17) 0.66505(9) 0.28366(13) 0.0393(6) Uani 1 1 d . . . . .
H33A H 0.657189 0.638507 0.320808 0.047 Uiso 1 1 calc R U . . .
H33B H 0.700493 0.643385 0.237979 0.047 Uiso 1 1 calc R U . . .
C46 C 0.78039(17) 0.74686(10) 0.17439(13) 0.0400(6) Uani 1 1 d . . . . .
H46 H 0.760930 0.709049 0.165442 0.048 Uiso 1 1 calc R U . . .
C8 C 0.5355(2) 0.57681(10) 0.52867(14) 0.0429(6) Uani 1 1 d . . . . .
H8 H 0.546223 0.537708 0.528431 0.051 Uiso 1 1 calc R U . . .
C49 C 0.29833(18) 0.71691(10) 0.23353(14) 0.0407(6) Uani 1 1 d . . . . .
C43 C 0.84023(17) 0.85707(11) 0.20032(13) 0.0427(6) Uani 1 1 d . . . . .
H43 H 0.861502 0.894586 0.209566 0.051 Uiso 1 1 calc R U . . .
C65 C 0.20554(19) 0.75606(11) 0.53048(15) 0.0461(6) Uani 1 1 d . . . . .
H65 H 0.198613 0.794020 0.544317 0.055 Uiso 1 1 calc R U . . .
C22 C 0.8283(2) 0.93572(10) 0.62561(14) 0.0485(7) Uani 1 1 d . . . . .
H22 H 0.887858 0.954288 0.651733 0.058 Uiso 1 1 calc R U . . .
C69 C 0.26978(18) 0.85539(10) 0.44628(14) 0.0431(6) Uani 1 1 d . . . . .
H69A H 0.222599 0.823351 0.433061 0.052 Uiso 1 1 calc R U . . .
H69B H 0.281267 0.873314 0.396092 0.052 Uiso 1 1 calc R U . . .
C44 C 0.89627(19) 0.82262(12) 0.15709(14) 0.0496(7) Uani 1 1 d . . . . .
H44 H 0.955101 0.836644 0.135457 0.060 Uiso 1 1 calc R U . . .
C54 C 0.22321(18) 0.75855(10) 0.24262(14) 0.0429(6) Uani 1 1 d . . . . .
C62 C 0.4812(2) 0.58185(9) 0.25449(14) 0.0457(6) Uani 1 1 d . . . . .
H62A H 0.435372 0.583682 0.203544 0.055 Uiso 1 1 calc R U . . .
H62B H 0.554219 0.579021 0.243100 0.055 Uiso 1 1 calc R U . . .
C68 C 0.2269(2) 0.64456(11) 0.49875(16) 0.0519(7) Uani 1 1 d . . . . .
H68 H 0.233461 0.605961 0.488567 0.062 Uiso 1 1 calc R U . . .
C57 C 0.2018(2) 0.91286(11) 0.20953(16) 0.0505(7) Uani 1 1 d . . . . .
H57 H 0.150742 0.941424 0.207782 0.061 Uiso 1 1 calc R U . . .
C45 C 0.86655(19) 0.76707(12) 0.14506(14) 0.0501(7) Uani 1 1 d . . . . .
H45 H 0.906375 0.743179 0.116358 0.060 Uiso 1 1 calc R U . . .
C58 C 0.30130(19) 0.92460(10) 0.19093(14) 0.0439(6) Uani 1 1 d . . . . .
H58 H 0.317308 0.960672 0.173273 0.053 Uiso 1 1 calc R U . . .
C56 C 0.17836(19) 0.86002(11) 0.23025(15) 0.0481(6) Uani 1 1 d . . . . .
H56 H 0.109716 0.852060 0.241245 0.058 Uiso 1 1 calc R U . . .
C50 C 0.2614(2) 0.66254(11) 0.21467(16) 0.0519(7) Uani 1 1 d . . . . .
H50 H 0.308571 0.634966 0.201110 0.062 Uiso 1 1 calc R U . . .
C66 C 0.1215(2) 0.72150(12) 0.52998(17) 0.0585(8) Uani 1 1 d . . . . .
H66 H 0.057101 0.735553 0.542703 0.070 Uiso 1 1 calc R U . . .
C67 C 0.1307(2) 0.66579(13) 0.51083(18) 0.0634(8) Uani 1 1 d . . . . .
H67 H 0.071111 0.642281 0.506014 0.076 Uiso 1 1 calc R U . . .
C53 C 0.1199(2) 0.74231(12) 0.24617(19) 0.0633(8) Uani 1 1 d . . . . .
H53 H 0.070481 0.769641 0.256723 0.076 Uiso 1 1 calc R U . . .
C63 C 0.4544(2) 0.52973(10) 0.29873(16) 0.0568(7) Uani 1 1 d . . . . .
H63A H 0.499462 0.528399 0.350084 0.068 Uiso 1 1 calc R U . . .
H63B H 0.470458 0.496553 0.268241 0.068 Uiso 1 1 calc R U . . .
C70 C 0.2137(2) 0.89715(11) 0.4938(2) 0.0675(9) Uani 1 1 d D . . . .
H70A H 0.256665 0.930997 0.505322 0.081 Uiso 0.645(7) 1 calc R U P A 1
H70B H 0.199505 0.880493 0.544169 0.081 Uiso 0.645(7) 1 calc R U P A 1
H70C H 0.243981 0.892641 0.549575 0.081 Uiso 0.355(7) 1 calc R U P A 2
H70D H 0.234061 0.934699 0.477559 0.081 Uiso 0.355(7) 1 calc R U P A 2
C64 C 0.3402(2) 0.52683(11) 0.31323(17) 0.0662(8) Uani 1 1 d . . . . .
H64A H 0.294844 0.529554 0.262873 0.099 Uiso 1 1 calc R U . . .
H64B H 0.325220 0.557677 0.347431 0.099 Uiso 1 1 calc R U . . .
H64C H 0.327503 0.491419 0.338661 0.099 Uiso 1 1 calc R U . . .
C51 C 0.1581(2) 0.64893(13) 0.2156(2) 0.0716(9) Uani 1 1 d . . . . .
H51 H 0.134961 0.612125 0.202912 0.086 Uiso 1 1 calc R U . . .
C52 C 0.0878(2) 0.68823(14) 0.2349(2) 0.0809(11) Uani 1 1 d . . . . .
H52 H 0.018137 0.677929 0.240252 0.097 Uiso 1 1 calc R U . . .
C71 C 0.1049(5) 0.9122(3) 0.4385(6) 0.103(3) Uani 0.645(7) 1 d D . P A 1
H71A H 0.120371 0.927150 0.387400 0.124 Uiso 0.645(7) 1 calc R U P A 1
H71B H 0.062581 0.878013 0.427948 0.124 Uiso 0.645(7) 1 calc R U P A 1
C34 C 0.0440(5) 0.9548(3) 0.4789(5) 0.138(4) Uani 0.645(7) 1 d D . P A 1
H34A H -0.026104 0.958719 0.449758 0.207 Uiso 0.645(7) 1 calc R U P A 1
H34B H 0.080087 0.990670 0.480463 0.207 Uiso 0.645(7) 1 calc R U P A 1
H34C H 0.038450 0.942465 0.532768 0.207 Uiso 0.645(7) 1 calc R U P A 1
C71A C 0.0987(6) 0.8979(3) 0.4923(5) 0.046(2) Uani 0.355(7) 1 d D . P A 2
H71C H 0.078672 0.924402 0.532000 0.055 Uiso 0.355(7) 1 calc R U P A 2
H71D H 0.073027 0.860456 0.504285 0.055 Uiso 0.355(7) 1 calc R U P A 2
C34A C 0.0529(7) 0.9156(5) 0.4112(6) 0.057(3) Uani 0.355(7) 1 d D . P A 2
H34D H 0.088701 0.949111 0.396236 0.085 Uiso 0.355(7) 1 calc R U P A 2
H34E H -0.021577 0.923540 0.410617 0.085 Uiso 0.355(7) 1 calc R U P A 2
H34F H 0.061650 0.885660 0.373792 0.085 Uiso 0.355(7) 1 calc R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O36 C27 1.379(2) . ?
O36 C35 1.441(2) . ?
O34 C16 1.380(2) . ?
O34 C33 1.426(3) . ?
C11 C6 1.423(3) . ?
C11 C12 1.463(3) . ?
C11 C10 1.405(3) . ?
C6 C5 1.454(3) . ?
C6 C7 1.413(3) . ?
C2 C1 1.391(3) . ?
C2 C3 1.440(3) . ?
C2 C69 1.523(3) . ?
C12 C13 1.446(3) . ?
C12 C3 1.413(3) . ?
C13 C14 1.480(3) . ?
C13 C26 1.405(3) . ?
C30 C29 1.471(3) . ?
C30 C38 1.430(3) . ?
C30 C31 1.404(3) . ?
C15 C14 1.405(3) . ?
C15 C16 1.379(3) . ?
C29 C28 1.409(3) . ?
C29 C41 1.398(3) . ?
C14 C19 1.410(3) . ?
C5 C4 1.418(3) . ?
C5 C68 1.400(3) . ?
C1 C26 1.425(3) . ?
C1 C35 1.523(3) . ?
C38 C60 1.473(3) . ?
C38 C37 1.406(3) . ?
C26 C25 1.459(3) . ?
C42 C47 1.408(3) . ?
C42 C41 1.464(3) . ?
C42 C43 1.411(3) . ?
C3 C4 1.467(3) . ?
C19 C20 1.457(3) . ?
C19 C18 1.410(3) . ?
C25 C20 1.407(3) . ?
C25 C24 1.412(3) . ?
C16 C17 1.393(3) . ?
C27 C39 1.396(3) . ?
C27 C28 1.373(3) . ?
C20 C21 1.405(3) . ?
C31 C47 1.466(3) . ?
C31 C32 1.430(3) . ?
C48 C32 1.393(3) . ?
C48 C37 1.438(3) . ?
C48 C61 1.524(3) . ?
C39 C40 1.377(3) . ?
C47 C46 1.405(3) . ?
C10 C9 1.383(3) . ?
C32 C33 1.537(3) . ?
C18 C17 1.370(3) . ?
C41 C40 1.404(3) . ?
C4 C65 1.411(3) . ?
C60 C55 1.406(3) . ?
C60 C59 1.401(3) . ?
C21 C22 1.374(3) . ?
C7 C8 1.363(3) . ?
C55 C54 1.461(3) . ?
C55 C56 1.409(3) . ?
C24 C23 1.380(3) . ?
C37 C49 1.480(3) . ?
C61 C62 1.538(3) . ?
C59 C58 1.365(3) . ?
C9 C8 1.392(3) . ?
C23 C22 1.383(3) . ?
C46 C45 1.369(3) . ?
C49 C54 1.417(3) . ?
C49 C50 1.414(3) . ?
C43 C44 1.378(3) . ?
C65 C66 1.366(3) . ?
C69 C70 1.533(3) . ?
C44 C45 1.397(3) . ?
C54 C53 1.400(3) . ?
C62 C63 1.527(3) . ?
C68 C67 1.384(3) . ?
C57 C58 1.393(3) . ?
C57 C56 1.364(3) . ?
C50 C51 1.376(3) . ?
C66 C67 1.387(4) . ?
C53 C52 1.371(4) . ?
C63 C64 1.529(4) . ?
C70 C71 1.630(8) . ?
C70 C71A 1.484(7) . ?
C51 C52 1.380(4) . ?
C71 C34 1.514(8) . ?
C71A C34A 1.499(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C27 O36 C35 118.35(15) . . ?
C16 O34 C33 118.55(16) . . ?
C6 C11 C12 119.88(19) . . ?
C10 C11 C6 117.75(19) . . ?
C10 C11 C12 122.32(19) . . ?
C11 C6 C5 119.03(19) . . ?
C7 C6 C11 118.5(2) . . ?
C7 C6 C5 121.8(2) . . ?
C1 C2 C3 118.98(19) . . ?
C1 C2 C69 119.12(19) . . ?
C3 C2 C69 121.60(19) . . ?
C13 C12 C11 122.17(19) . . ?
C3 C12 C11 119.44(18) . . ?
C3 C12 C13 118.32(18) . . ?
C12 C13 C14 125.63(18) . . ?
C26 C13 C12 118.58(18) . . ?
C26 C13 C14 115.10(17) . . ?
C38 C30 C29 125.06(18) . . ?
C31 C30 C29 115.59(18) . . ?
C31 C30 C38 118.39(18) . . ?
C16 C15 C14 121.0(2) . . ?
C28 C29 C30 119.86(18) . . ?
C41 C29 C30 120.25(18) . . ?
C41 C29 C28 118.75(19) . . ?
C15 C14 C13 120.68(19) . . ?
C15 C14 C19 118.73(19) . . ?
C19 C14 C13 119.62(18) . . ?
C4 C5 C6 119.07(19) . . ?
C68 C5 C6 121.5(2) . . ?
C68 C5 C4 118.8(2) . . ?
C2 C1 C26 120.33(19) . . ?
C2 C1 C35 118.7(2) . . ?
C26 C1 C35 119.63(18) . . ?
C30 C38 C60 120.83(19) . . ?
C37 C38 C30 119.17(19) . . ?
C37 C38 C60 120.00(19) . . ?
C13 C26 C1 117.14(19) . . ?
C13 C26 C25 117.70(19) . . ?
C1 C26 C25 125.07(19) . . ?
C47 C42 C41 118.03(19) . . ?
C47 C42 C43 119.8(2) . . ?
C43 C42 C41 122.1(2) . . ?
C2 C3 C4 122.51(19) . . ?
C12 C3 C2 118.72(18) . . ?
C12 C3 C4 118.55(19) . . ?
C14 C19 C20 119.02(19) . . ?
C14 C19 C18 118.74(19) . . ?
C18 C19 C20 122.1(2) . . ?
C20 C25 C26 120.06(18) . . ?
C20 C25 C24 118.4(2) . . ?
C24 C25 C26 121.3(2) . . ?
O34 C16 C17 115.24(19) . . ?
C15 C16 O34 124.5(2) . . ?
C15 C16 C17 120.2(2) . . ?
O36 C27 C39 115.25(19) . . ?
C28 C27 O36 124.23(19) . . ?
C28 C27 C39 120.46(19) . . ?
C25 C20 C19 117.8(2) . . ?
C21 C20 C19 123.0(2) . . ?
C21 C20 C25 119.2(2) . . ?
C30 C31 C47 117.25(19) . . ?
C30 C31 C32 117.46(18) . . ?
C32 C31 C47 125.17(19) . . ?
C32 C48 C37 118.54(19) . . ?
C32 C48 C61 120.2(2) . . ?
C37 C48 C61 120.74(19) . . ?
C40 C39 C27 119.2(2) . . ?
C42 C47 C31 119.81(18) . . ?
C46 C47 C42 118.4(2) . . ?
C46 C47 C31 121.2(2) . . ?
C9 C10 C11 121.8(2) . . ?
C31 C32 C33 118.76(19) . . ?
C48 C32 C31 120.41(19) . . ?
C48 C32 C33 119.12(19) . . ?
C27 C28 C29 120.88(19) . . ?
C17 C18 C19 121.5(2) . . ?
C29 C41 C42 118.47(19) . . ?
C29 C41 C40 119.28(19) . . ?
C40 C41 C42 122.0(2) . . ?
C5 C4 C3 120.14(19) . . ?
C65 C4 C5 117.6(2) . . ?
C65 C4 C3 122.2(2) . . ?
C39 C40 C41 121.3(2) . . ?
C18 C17 C16 119.6(2) . . ?
C55 C60 C38 119.41(19) . . ?
C59 C60 C38 122.31(19) . . ?
C59 C60 C55 118.3(2) . . ?
C22 C21 C20 121.1(2) . . ?
C8 C7 C6 121.9(2) . . ?
C60 C55 C54 119.5(2) . . ?
C60 C55 C56 118.0(2) . . ?
C56 C55 C54 122.0(2) . . ?
C23 C24 C25 121.2(2) . . ?
C38 C37 C48 118.9(2) . . ?
C38 C37 C49 117.80(19) . . ?
C48 C37 C49 122.82(19) . . ?
C48 C61 C62 117.79(17) . . ?
C58 C59 C60 122.1(2) . . ?
O36 C35 C1 115.35(17) . . ?
C10 C9 C8 119.7(2) . . ?
C24 C23 C22 119.8(2) . . ?
O34 C33 C32 115.56(18) . . ?
C45 C46 C47 121.2(2) . . ?
C7 C8 C9 119.8(2) . . ?
C54 C49 C37 120.2(2) . . ?
C50 C49 C37 122.3(2) . . ?
C50 C49 C54 117.5(2) . . ?
C44 C43 C42 120.1(2) . . ?
C66 C65 C4 122.0(2) . . ?
C21 C22 C23 120.3(2) . . ?
C2 C69 C70 116.6(2) . . ?
C43 C44 C45 120.0(2) . . ?
C49 C54 C55 118.6(2) . . ?
C53 C54 C55 122.1(2) . . ?
C53 C54 C49 118.6(2) . . ?
C63 C62 C61 113.01(18) . . ?
C67 C68 C5 121.2(3) . . ?
C56 C57 C58 119.4(2) . . ?
C46 C45 C44 120.4(2) . . ?
C59 C58 C57 119.5(2) . . ?
C57 C56 C55 122.1(2) . . ?
C51 C50 C49 121.1(3) . . ?
C65 C66 C67 119.7(2) . . ?
C68 C67 C66 119.8(3) . . ?
C52 C53 C54 122.1(3) . . ?
C62 C63 C64 113.8(2) . . ?
C69 C70 C71 105.5(4) . . ?
C71A C70 C69 122.8(4) . . ?
C50 C51 C52 120.6(3) . . ?
C53 C52 C51 119.1(3) . . ?
C34 C71 C70 110.1(7) . . ?
C70 C71A C34A 107.0(6) . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 406.4 131.5 '2 hexane'
2 0.000 0.500 0.500 406.4 131.5 '2 hexane'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.175
_oxdiff_exptl_absorpt_empirical_full_min 0.778
